CN105973880B - The instant test paper and its application method of a kind of rapid evaluation aluminum in food constituent content and application - Google Patents
The instant test paper and its application method of a kind of rapid evaluation aluminum in food constituent content and application Download PDFInfo
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
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Abstract
The present invention relates to a kind of instant test paper of rapid evaluation aluminum in food constituent content, making step is as follows: preparing 1% sulfuric acid solution；Prepare acetic acid-sodium acetate solution；Prepare 3% acetic acid solution；Prepare cetrimonium bronmide solution；Prepare chrome azurol S solution；The production of colour developing test paper；The production of standard color comparison card；Up to instant test paper.This test paper is based on chrome azurol S method and detects aluminium content method, it is main to utilize in the range of PH6.7~7.0, aluminium reacts in the presence of bromohexadecane base trimethylamine with chrome azurol S, au bleu, carry out colorimetric assay, the test paper being capable of aluminium content in rapid and accurate determination food, better assure that the physical safety of consumer, improve the accuracy of the safety index of detection food, strengthen food products market supervision, be of great significance, meanwhile, the test paper have the advantages that small in size, Portable belt, it is easy to detect, at low cost, convenient for universal.
Description
Technical field
The invention belongs to technical field of food safety detection, especially a kind of rapid evaluation aluminum in food constituent content is
With type test paper and its application method and application.
Background technique
Aluminium and its compound are generally existing in the environment, are the metallic elements that content is most in the earth's crust, since it is with excellent
Good physicochemical property, aluminium and its correlated product are widely used in daily life and production, thus the aluminium exposure in crowd is
Inevitably.Epidemiological studies are it is demonstrated experimentally that the aluminium of long-time excess intake causes apparent nervous function to change
Become, and influences intellectual development；When aluminium content is more than 5-10 times of aluminium content in general diet in food, so that it may cause bone soft
Change and fracture, to make skeletogenous damage and deformation, the diseases such as osteomalacia, osteoporosis occur.In addition, a large amount of science
Experimental studies have found that the aluminium of long-time excess intake to human reproductive systems, hemopoietic system, immune system, liver, lung, kidney, bone,
Heart etc. generates chronic murder by poisoning, but people usually ignore the presence and its chronic toxicity of aluminium in daily life.According to calculating,
As soon as individual weight is the adult weekly such as consumption 255g deep-fried twisted dough sticks of 55kg, diet aluminium intake is more than to fix tentatively to can tolerate intake weekly
It measures (PTWI).So accurately and rapidly measurement aluminium content is to guarantee the important prerequisite of consumer safety.
Therefore, the test paper for developing a kind of rapid and accurate determination Aluminum Content in Food, for better ensuring that the body of consumer
Body safety, the safety index of detection food, reinforcement food products market supervision are of great significance.
The detection method of current existing aluminium has very much, such as: spectrophotometry, graphite furnace atomic absorption spectrometry, mass spectrum
Method, inductive coupling plasma emission spectrum method etc., they need expensive instrument and complicated for operation, special technology people mostly
Member, and detection cycle is long, costly, cannot achieve on-site test and popularizes.And test paper examines detection technique to have test paper volume
Small, Portable belt, it is easy to detect, at low cost the features such as, be it is a kind of can be applied to everyday home life in quickly and accurately inspection
Survey the detection method of food and Aluminium in Drinking Water content.
By retrieval, following two patent publication us relevant to present patent application are found:
1, aluminium ion Test paper and preparation method thereof and application method (CN103499574A), the Test paper is using filter
Paper takes out after infiltrating in maceration extract, is made after dry, the maceration extract includes 0.1-0.6 grams of chrome azurol S and dissolves in 100 milliliters of steamings
In distilled water, 0.5 gram of uniform mixed preparing maceration extract I and ascorbic acid and 2 grams of Phen successively dissolve in 100 milliliters of distilled water
The maceration extract II of uniform mixed preparing；The Test paper cooperates molten by 0.2mol/L disodium hydrogen phosphate using chrome azurol S as color developing agent
Liquid 12.64mL is uniformly mixed the activator being configured to 0.1mol/L citric acid solution 7.37mL and uses, and makes simple, at low cost
It is honest and clean, it is easy to use, free from environmental pollution, it is environmental；Test scope is wide, operates without professional, especially suitable for quickly existing
Field detecting aluminium content.
2, a kind of test paper for aluminium content detection and its preparation method and application (CN103913455A), the test paper,
Including carrier and developer, the carrier has water imbibition, and the color developing agent is adsorbed almost uniformly on the carrier, described aobvious
Toner is chrome azurol S.The test paper using simple immersion process prepare, can be used for the quick detection of aluminium content, have quickly,
Advantage sensitive, easy to operate, low in cost, and operated without professional, it is particularly suitable for illegally adding in edible jelly fungi
The quick detection of aluminum phosphate, voluntarily uses in the family convenient for the common people, can also be used for the quick real-time inspection of food safety, market
It surveys.
By comparison, there is essential difference in present patent application and above-mentioned patent publication us.
Summary of the invention
It is an object of the invention in place of overcome the deficiencies in the prior art, provide a kind of rapid evaluation aluminum in food element to contain
The instant test paper and its application method of amount and application, when carrying out the detection of Aluminum Content in Food using the test paper, sample treatment
Mode is simple and efficient, efficient measurement, low in cost, test result is accurate, convenient for universal, which can be widely applied to eat
The detection of aluminium content in product.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of instant test paper of rapid evaluation aluminum in food constituent content, making step are as follows:
(1) prepare 1% sulfuric acid solution: drawing 1mol/L sulfuric acid and be diluted with water, until sulfuric acid, which is added, accounts for overall solution volume
Percentage by volume be 1-3%, obtain 1% sulfuric acid solution；
(2) prepare acetic acid-sodium acetate solution: weigh the sodium acetate mass concentration soluble in water to sodium acetate be 0.075~
Then glacial acetic acid is added in 0.076g/mL, adjust pH to 5-5.5, and the mass concentration for being then diluted with water to sodium acetate is 0.068g/
ML obtains acetic acid-sodium acetate solution；
The sodium acetate: the ratio g:mL of glacial acetic acid is 17:1.3-1.5；
(3) prepare 3% acetic acid solution: drawing the percentage by volume that glacial acetic acid is slowly added into ultrapure water to glacial acetic acid is
3%, it then mixes, obtains 3% acetic acid solution；
(4) prepare cetrimonium bronmide solution: weighing cetrimonium bronmide and be diluted with water to bromination 16
The concentration of alkyl trimethylamine is 0.2-0.25g/L, obtains cetrimonium bronmide solution；
(5) prepare chrome azurol S solution: weighing chrome azurol S and being diluted with water to the concentration of chrome azurol S is 0.5-0.6g/L, obtains chromium
Reddish black S solution；
(6) the production of colour developing test paper: by 1% sulfuric acid solution, acetic acid-sodium acetate solution, 3% acetic acid solution, bromination ten
Six alkyl trimethylamine solutions, chrome azurol S solution are mixed and made into soak according to the ratio that volume ratio is 1:5:1:1:1, by test paper
Carrier is cut into the long width that multiplies and impregnates in soak 3-5 hours for the rectangle of 4.5-5.5cm × 0.8-1.2cm, 50 DEG C of vacuum perseverances
The dry 4h of temperature, saves, obtains colour developing test paper；
The test paper carrier is chromatography filter paper；
(7) the production of standard color comparison card: by the aluminum standard solution drop of various concentration on colour developing test paper, chromogenic reaction occurs
After 1-3 minutes, color is taken with color difference meter, standard color comparison card is made；
(8) up to instant test paper.
Moreover, making step is as follows:
(1) prepare 1% sulfuric acid solution: drawing 1mol/L sulfuric acid and be diluted with water, until sulfuric acid, which is added, accounts for overall solution volume
Percentage by volume be 1%, obtain 1% sulfuric acid solution；
(2) prepare acetic acid-sodium acetate solution: weigh the sodium acetate mass concentration soluble in water to sodium acetate be 0.075~
Then glacial acetic acid is added in 0.076g/mL, adjust pH to 5.5, and the mass concentration for being then diluted with water to sodium acetate is 0.068g/mL,
Obtain acetic acid-sodium acetate solution；
The sodium acetate: the ratio g:mL of glacial acetic acid is 17:1.3；
(3) prepare 3% acetic acid solution: drawing the percentage by volume that glacial acetic acid is slowly added into ultrapure water to glacial acetic acid is
3%, it then mixes, obtains 3% acetic acid solution；
(4) prepare cetrimonium bronmide solution: weighing cetrimonium bronmide and be diluted with water to bromination 16
The concentration of alkyl trimethylamine is 0.2g/L, obtains cetrimonium bronmide solution；
(5) prepare chrome azurol S solution: weighing chrome azurol S and being diluted with water to the concentration of chrome azurol S is 0.5g/L, obtains chromazurine
S solution；
(6) the production of colour developing test paper: by 1% sulfuric acid solution, acetic acid-sodium acetate solution, 3% acetic acid solution, bromination ten
Six alkyl trimethylamine solutions, chrome azurol S solution are mixed and made into soak according to the ratio that volume ratio is 1:5:1:1:1, by test paper
Carrier is cut into the long width that multiplies and impregnates in soak 4 hours for the rectangle of 5cm × 1cm, and the dry 4h of 50 DEG C of vacuum constant temperatures are saved,
Must develop the color test paper；
The test paper carrier is chromatography filter paper；
(7) the production of standard color comparison card: the aluminium standard of various concentration 0.25g/L, 0.5g/L, 1g/L, 2g/L, 4g/L is molten
Drop after chromogenic reaction occurs 1 minute, takes color with color difference meter, standard color comparison card is made on through colour developing test paper；
(8) up to instant test paper.
Moreover, the step (5) in chrome azurol S concentration optimization method it is as follows:
Based on the chrome azurol S compound concentration in national standard GB/T5009.182-2003, except the 0.5g/L of national regulations
Outside concentration, the chrome azurol S concentration of 0.25g/L, 1g/L, 2g/L and 4g/L are also separately designed, according to visually observing readability
Select most suitable chrome azurol S concentration to get 0.5g/L；
Alternatively, the optimization method of the step (6) pilot scale paper carrier is as follows:
A4 paper, common quantitative filter paper and chromatography filter paper is used to carry out as test paper carrier by the production method of instant test paper
Production, and by aluminum standard solution drop on test paper carrier, observing colour developing area and color developing effect on each test paper carrier, and select
Most suitable test paper carrier, i.e. chromatography filter paper out；
Alternatively, the step (6) in colour developing test paper drying mode optimization method it is as follows:
Choosing natural drying, freeze-day with constant temperature and the dry three kinds of drying modes of vacuum constant temperature, the flatness, color of paper after drying
And miscellaneous spot situation determines optimum drying condition, i.e. vacuum drying 50 DEG C, 4h；
Alternatively, (7) the middle optimization method for observing the testing result time is as follows for the step:
With aluminum standard solution drop on test paper, the colour developing situation of test paper after observation different time 0.5-60 minutes is determined most
After good observation testing result time, i.e. chromogenic reaction occur 1 minute.
The application method of the instant test paper of rapid evaluation aluminum in food constituent content as described above, steps are as follows:
It is added to the water after food is shredded, the ratio g:mL of food and water is 1:5-12, and adding percentage by volume is 3%
Acetic acid, the ratio g:mL of the food and acetic acid is 1:1-3；With taking immersion drop after 30-60 DEG C of water-bath heating 1-60 minutes
On display test paper, observing response area color, and compared with standard color comparison card, the inspection to aluminium content is realized according to the depth of color
It surveys.
Moreover, the detection method of the aluminum in food constituent content is as follows:
It is added to the water after food is shredded, the ratio g:mL of food and water is 1:9, and adding percentage by volume is 3%
The ratio g:mL of acetic acid, the food and acetic acid is 1:1；Immersion drop is taken to exist after being heated 30-50 minutes with 40 DEG C of immersions of water-bath
It shows on test paper, observing response area color, and is compared with standard color comparison card, the inspection to aluminium content is realized according to the depth of color
It surveys, the whether qualified regulation according to national standard of the aluminium element content in the food of detection is judged.
Moreover, the condition optimizing of the food pre-treatment is as follows:
Food is divided into 8 groups, the ratio g:mL for being separately added into food and acetic acid is 0,10:1,5:1,2:1,1:1,1:4,1:
8, the ethyl alcohol that the percentage by volume of 1:10 is 3%, selects most suitable 3% acetic acid additional amount, and the ratio g:mL of instant food and acetic acid is
1:1；
The food of most suitable 3% acetic acid additional amount will be added, with 25-100 DEG C of water-bath heating 1-60 minutes, in different temperatures
Sample detection at 25-100 DEG C observes the leaching content of its aluminium, selects the water-bath soaking temperature of most suitable food, as 40 DEG C；
The food of the most suitable 3% acetic acid additional amount heated at constant temperature under the water-bath soaking temperature of most suitable food will be added, not
With time 1-60 minute sample detection, the aluminium leaching content of sample is observed, selects the heating time of most suitable food, as 30 minutes.
The instant test paper of rapid evaluation aluminum in food constituent content as described above is in Rapid determination of aluminum in food content
In application.
Moreover, the food is jellyfish or deep-fried twisted dough sticks.
The advantages of present invention obtains and good effect are:
1, test paper of the present invention is based on chrome azurol S method and detects aluminium content method, main to utilize the aluminium in the range of PH6.7~7.0
It is reacted in the presence of bromohexadecane base trimethylamine with chrome azurol S, au bleu, carries out colorimetric assay, which focuses on exploitation
A kind of method of simple and efficient detection aluminium content, the test paper can aluminium content in rapid and accurate determination food, preferably protect
The physical safety for having demonstrate,proved consumer improves the accuracy of the safety index of detection food, strengthens food products market supervision, has
Significance, meanwhile, the test paper have the advantages that small in size, Portable belt, it is easy to detect, at low cost, convenient for universal.
2, test paper of the present invention is slowly added into the body in ultrapure water to glacial acetic acid using absorption glacial acetic acid during the preparation process
Product percentage is 3%, mixes, to simulate light-coloured vinegar common in daily life, realizes under home environment to food materials aluminium content
Real-time monitoring, it is extremely easy to use, improve the use scope of the test paper.
3, test paper of the present invention is during the preparation process compared the test paper after immersion and oneself using vacuum drying drying mode
Right drying and heated-air drying, test paper surfacing corrugationless, without obvious locus coeruleus, impurity effect is small, achieves unexpected skill
Art effect.
4, the method for test paper of the present invention assessment aluminum in food constituent content is easy to operate, do not need expensive large machines and
Professional, can test operation completely at home conditions, reduce testing cost, improve the convenience of detection, pole
The earth facilitates detection.
5, the pre-treating method of test paper of the present invention and detected food makes the detection and conventional method of Aluminum Content in Food
It compares, more fast, and has the recovery of standard addition (94.6%-105.8%) of preferable minimum quantitative limit (0.5mg/L), to leaching
Steep the detection and the ICP-MS method result goodness of fit with higher of aluminium in liquid, the equation after two methods detected value linear fit
Are as follows: Y=1.0159x-0.0724, R2=0.9624.
Detailed description of the invention
Fig. 1 is test paper carriers different in the present invention to aluminum solutions reaction solution situation map；
Fig. 2 is different chromogenic agents and Al in the present invention3+Solution reaction colour developing situation map；
Fig. 3 is the colour developing situation map of different developing times in the present invention；
Influence diagram of the different acid adding amounts of food to leaching content when Fig. 4 is test paper detection in the present invention；
Influence diagram of the different heating soaking temperature of food to leaching content when Fig. 5 is test paper detection in the present invention；
Influence diagram of the different heating soaking time of food to leaching rate when Fig. 6 is test paper detection in the present invention；
Fig. 7 is Plays colorimetric card pattern of the present invention；
Fig. 8 is the Linear Fit Chart of soak test paper testing result and ICP-MS testing result in the present invention.
Specific embodiment
Below with reference to embodiment, the present invention is further described；Following embodiments be it is illustrative, be not restrictive,
It cannot be limited the scope of protection of the present invention with following embodiments.
Raw material used in the present invention is unless otherwise specified conventional commercial product；Used in the present invention
Method is unless otherwise specified the conventional method of this field.
Embodiment 1
A kind of instant test paper of rapid evaluation aluminum in food constituent content, making step are as follows:
(1) prepare 1% sulfuric acid solution: drawing 1mol/L sulfuric acid and be diluted with water, until sulfuric acid, which is added, accounts for overall solution volume
Percentage by volume be 1-3%, obtain 1% sulfuric acid solution；
(2) prepare acetic acid-sodium acetate solution: weigh the sodium acetate mass concentration soluble in water to sodium acetate be 0.075~
Then glacial acetic acid is added in 0.076g/mL, adjust pH to 5-5.5, and the mass concentration for being then diluted with water to sodium acetate is 0.068g/
ML obtains acetic acid-sodium acetate solution；
The sodium acetate: the ratio g:mL of glacial acetic acid is 17:1.3-1.5；
(3) prepare 3% acetic acid solution: drawing the percentage by volume that glacial acetic acid is slowly added into ultrapure water to glacial acetic acid is
3%, it then mixes, obtains 3% acetic acid solution；
(4) prepare cetrimonium bronmide solution: weighing cetrimonium bronmide and be diluted with water to bromination 16
The concentration of alkyl trimethylamine is 0.2-0.25g/L, obtains cetrimonium bronmide solution；
(5) prepare chrome azurol S solution: weighing chrome azurol S and being diluted with water to the concentration of chrome azurol S is 0.5-0.6g/L, obtains chromium
Reddish black S solution；
(6) the production of colour developing test paper: by 1% sulfuric acid solution, acetic acid-sodium acetate solution, 3% acetic acid solution, bromination ten
Six alkyl trimethylamine solutions, chrome azurol S solution are mixed and made into soak according to the ratio that volume ratio is 1:5:1:1:1, by test paper
Carrier is cut into the long width that multiplies and impregnates in soak 3-4 hours for the rectangle of 4.5-5.5cm × 0.8-1.2cm, 50 DEG C of vacuum perseverances
The dry 4h of temperature, saves, obtains colour developing test paper；
The test paper carrier is chromatography filter paper；
(7) the production of standard color comparison card: by the aluminum standard solution drop of various concentration on colour developing test paper, chromogenic reaction occurs
After 1-3 minutes, color is taken with color difference meter, standard color comparison card is made；
(8) up to instant test paper.
More preferably, the instant test paper of above-mentioned rapid evaluation aluminum in food constituent content, making step are as follows:
(1) prepare 1% sulfuric acid solution: drawing 1mol/L sulfuric acid and be diluted with water, until sulfuric acid, which is added, accounts for overall solution volume
Percentage by volume be 1%, obtain 1% sulfuric acid solution；
(2) prepare acetic acid-sodium acetate solution: weigh the sodium acetate mass concentration soluble in water to sodium acetate be 0.075~
Then glacial acetic acid is added in 0.076g/mL, adjust pH to 5.5, and the mass concentration for being then diluted with water to sodium acetate is 0.068g/mL,
Obtain acetic acid-sodium acetate solution；
The sodium acetate: the ratio g:mL of glacial acetic acid is 17:1.3；
(3) prepare 3% acetic acid solution: drawing the percentage by volume that glacial acetic acid is slowly added into ultrapure water to glacial acetic acid is
3%, it then mixes, obtains 3% acetic acid solution；
(4) prepare cetrimonium bronmide solution: weighing cetrimonium bronmide and be diluted with water to bromination 16
The concentration of alkyl trimethylamine is 0.2g/L, obtains cetrimonium bronmide solution；
(5) prepare chrome azurol S solution: weighing chrome azurol S and being diluted with water to the concentration of chrome azurol S is 0.5g/L, obtains chromazurine
S solution；
(6) the production of colour developing test paper: by 1% sulfuric acid solution, acetic acid-sodium acetate solution, 3% acetic acid solution, bromination ten
Six alkyl trimethylamine solutions, chrome azurol S solution are mixed and made into soak according to the ratio that volume ratio is 1:5:1:1:1, by test paper
Carrier is cut into the long width that multiplies and impregnates in soak 4 hours for the rectangle of 5cm × 1cm, and the dry 4h of 50 DEG C of vacuum constant temperatures are saved,
Must develop the color test paper；
The test paper carrier is chromatography filter paper；
(7) the production of standard color comparison card: the aluminium standard of various concentration 0.25g/L, 0.5g/L, 1g/L, 2g/L, 4g/L is molten
Drop after chromogenic reaction occurs 1 minute, takes color with color difference meter, standard color comparison card is made on colour developing test paper；
(8) up to instant test paper.
The step (5) in the optimization method of concentration of chrome azurol S can be such that
Based on the chrome azurol S compound concentration in national standard GB/T5009.182-2003, it is contemplated that be visually observed
Color sensitivity it is low, test strips contacted with air can make Some Drugs aoxidize and fail etc. factors, remove national regulations
0.5g/L concentration outside, the chrome azurol S concentration of 0.25g/L, 1g/L, 2g/L and 4g/L have also been separately designed, according to visually observing
Readability selects most suitable chrome azurol S concentration to get 0.5g/L；
Alternatively, the optimization method of the step (6) pilot scale paper carrier is as follows:
A4 paper, common quantitative filter paper and chromatography filter paper is used to carry out as test paper carrier by the production method of instant test paper
Production, and by aluminum standard solution drop on test paper carrier, observing colour developing area and color developing effect on each test paper carrier, and select
Most suitable test paper carrier, i.e. chromatography filter paper out；
Alternatively, the step (6) in colour developing test paper drying mode optimization method it is as follows:
Choosing spontaneously dries, freeze-day with constant temperature and the dry three kinds of drying modes of vacuum constant temperature, different drying modes are shown in Table 1, from
The flatness, color and miscellaneous spot situation of paper determine optimum drying condition after drying, i.e. vacuum drying 50 DEG C, 4h；
Alternatively, (7) the middle optimization method for observing the testing result time is as follows for the step:
With aluminum standard solution drop on test paper, the colour developing situation of different time 0.5-60 minutes test paper is observed, is determined best
The testing result time is observed, i.e., after chromogenic reaction occurs 1 minute.
The application method of the instant test paper of rapid evaluation aluminum in food constituent content as described above, steps are as follows:
It is added to the water after food is shredded, the ratio g:mL of food and water is 1:5-12, and adding percentage by volume is 3%
Acetic acid, the ratio g:mL of the food and acetic acid is 1:1-3；With taking immersion drop after 30-60 DEG C of water-bath heating 1-60 minutes
On display test paper, observing response area color, and compared with standard color comparison card, the inspection to aluminium content is realized according to the depth of color
It surveys.
Further, the detection method of the aluminum in food constituent content is as follows:
It is added to the water after food is shredded, the ratio g:mL of food and water is 1:9, and adding percentage by volume is 3%
The ratio g:mL of acetic acid, the food and acetic acid is 1:1；Immersion drop is taken to exist after being heated 30-50 minutes with 40 DEG C of immersions of water-bath
It shows on test paper, observing response area color, and is compared with standard color comparison card, the inspection to aluminium content is realized according to the depth of color
It surveys, the whether qualified regulation according to national standard of the aluminium element content in the food of detection is judged.
Further, the condition optimizing of the food pre-treatment is as follows: food being divided into 8 groups, is separately added into food and acetic acid
Ratio g:mL be 0, the ethyl alcohol that the percentage by volume of 10:1,5:1,2:1,1:1,1:4,1:8,1:10 are 3%, select most suitable
The ratio g:mL of 3% acetic acid additional amount, instant food and acetic acid is 1:1；
The food of most suitable 3% acetic acid additional amount will be added, is heated 30 minutes with 25-100 DEG C of water-bath, in different temperatures 25-
Sample detection at 100 DEG C observes the leaching content of its aluminium, selects the water-bath soaking temperature of most suitable food, as 40 DEG C；
The food of the most suitable 3% acetic acid additional amount heated at constant temperature under the water-bath soaking temperature of most suitable food will be added, not
With time 1-60 minute sample detection, the aluminium leaching content of sample is observed, selects the heating time of most suitable food, i.e., 30 minutes.
The instant test paper of above-mentioned rapid evaluation aluminum in food constituent content can be applied in Rapid determination of aluminum in food
In content, such as apply the detection of the aluminium content in jellyfish or deep-fried twisted dough sticks.
Embodiment 2
A kind of instant test paper of rapid evaluation aluminum in food constituent content, making step are as follows:
One, the preparation of solution early period
1, it 1% sulfuric acid solution: draws 1mL1mol/L sulfuric acid and is diluted with water to 100mL scale.
2, acetic acid-sodium acetate solution: weighing 34g sodium acetate and be dissolved in 450mL water, adds 2.6mL glacial acetic acid, adjusts pH extremely
5.5, it is diluted with water to 500mL.
3, it 3% acetic acid solution: draws 3mL glacial acetic acid and is slowly added into 97mL ultrapure water, mix (to simulate daily life
Common light-coloured vinegar in work).
4, it cetrimonium bronmide solution: weighs 20mg cetrimonium bronmide and is diluted with water to 100mL quarter
Degree, this solution 0.2g/L.
5, chrome azurol S solution: weighing 50mg chrome azurol S and be diluted with water to 100mL scale, this solution 0.5g/L.
Two, the manufacturing conditions optimization of test paper
By selected test paper carrier be cut into it is long multiply the rectangle that width is 5cm × 1cm, through drying after being impregnated in reaction solution,
And it saves.
The optimization method of the test paper carrier is as follows:
A4 paper, common quantitative filter paper and chromatography filter paper is used to carry out as test paper carrier by the production method of instant test paper
Production, and by aluminum standard solution drop on test paper carrier, observing colour developing area and color developing effect on each test paper carrier, and select
Most suitable test paper carrier, i.e. chromatography filter paper out, the result is shown in Figure 1, with A4 paper, common quantitative filter paper and chromatography filter paper and various concentration
Al3+ solution reaction.From the point of view of the situation that develops the color, chromatography filter paper keeps the aluminium color range of various concentration more apparent, and A4 paper reaction solution is spread not
Uniformly and suction dose is few, and common quantitative filter paper inhales dose and chromatography filter paper is very nearly the same, but gradient color developing effect is compared with chromatography filter paper
Difference；
The optimization method of the concentration of the chrome azurol S is as follows:
Based on the chrome azurol S compound concentration in national standard GB/T5009.182-2003, it is contemplated that be visually observed
Color sensitivity it is low, test strips contacted with air can make Some Drugs aoxidize and fail etc. factors, therefore remove national standard
Outside defined 0.5g/L concentration, the chrome azurol S concentration of 0.25g/L, 1g/L, 2g/L and 4g/L are also separately designed, according to naked eyes
Observing readability selects most suitable chrome azurol S concentration to get 0.5g/L, as a result sees that Fig. 2 0.5g/L concentration develops the color compared with other concentration
Effect is good, convenient for visually observing；
The optimization method of the drying mode of the colour developing test paper is as follows:
Choosing natural drying, freeze-day with constant temperature and the dry three kinds of drying modes of vacuum constant temperature, the flatness, color of paper after drying
And miscellaneous spot situation determines optimum drying condition, i.e. vacuum drying 50 DEG C, 4h, processing mode and the results are shown in Table 1, is tried repeatedly
It tests, vacuum drying can exclude influence of most of introduced contaminants to test paper, and test paper appearance is best when temperature is 50 DEG C, when dry
Between 4h.Therefore the dry optimum condition of test paper is the dry 4h of 50 DEG C of vacuum constant temperatures；
(7) the middle optimization method for observing the testing result time is as follows for the step:
With aluminum standard solution drop on test paper, observation different time 0.5min, 1min, 2min, 3min, 5min, 10min,
The colour developing situation of test paper after 20min, 30min, 60min, determines the optimal viewing testing result time, i.e. chromogenic reaction occurs 1 point
As a result Zhong Hou is shown in Fig. 3, test paper color development area color is similar between developing time 30s~2min, and after 2min, develop the color area's face
Color shoals increase with time, is unfavorable for visually observing.Consider to guarantee the color developing agent fully reacting on aluminium and test paper, choosing colour developing eventually
Time is 1min.
Influence table of the different drying modes of table 1 to test paper
Table 1 is the results show that through repetition test, and naturally dry needs 7h, and drying time is too long, affected by environment larger, examination
Paper quality is unstable；Test paper is affected under the conditions of freeze-day with constant temperature by drying temperature, and test paper quality is low；Vacuum drying can arrange
Influence except most of introduced contaminants to test paper, test paper appearance is best when temperature is 50 DEG C, drying time 4h.
The result shows that the dry optimum condition of test paper is the dry 4h of 50 DEG C of vacuum constant temperatures.
Three, the production of instant test paper:
1, the production of colour developing test paper: by 1% sulfuric acid solution, acetic acid-sodium acetate solution, 3% acetic acid solution, bromination ten
Six alkyl trimethylamine solutions, chrome azurol S solution are mixed and made into soak according to the ratio that volume ratio is 1:5:1:1:1, by test paper
Carrier is cut into the long width that multiplies and impregnates in soak 4-5 hours for the rectangle of 4.5-5.5cm × 0.8-1.2cm, 50 DEG C of vacuum perseverances
The dry 4h of temperature, saves, obtains colour developing test paper；
The test paper carrier is chromatography filter paper；
2, the production of standard color comparison card: by the aluminum standard solution drop of various concentration on colour developing test paper, chromogenic reaction occurs
After 1-3 minutes, color is taken with color difference meter, standard color comparison card is made to get instant test paper.
Four, food samples Pretreatment optimizes
Food is divided into 8 groups, the ratio g:mL for being separately added into food and acetic acid is 0,10:1,5:1,2:1,1:1,1:4,1:
8, the ethyl alcohol that the percentage by volume of 1:10 is 3%, selects most suitable 3% acetic acid additional amount, and the ratio g:mL of instant food and acetic acid is
As a result 1:1 is shown in Fig. 4, be within the scope of 0~5mL in 3% acetic acid dosage, the leaching rate of aluminium increases sharply with the increase of acid adding amount.
It is within the scope of 5~50mL in 3% acetic acid dosage, as acetic acid dosage steps up, the leaching rate of aluminium tends to be steady.
The food of most suitable 3% acetic acid additional amount will be added, with 25-100 DEG C of water-bath heating 1-60 minutes, in different temperatures
Sample detection at 25-100 DEG C observes the leaching content of its aluminium, as a result 40 DEG C of water-bath soaking temperature for selecting most suitable food are shown in Fig. 5,
It is room temperature (24 DEG C) within the scope of 60 DEG C in soaking temperature, aluminium leaching rate gradually rises with the raising of temperature, in soaking temperature
For within the scope of 60~100 DEG C, with the raising of soaking temperature, the leaching rate of aluminium declines, leached in 80~100 DEG C of soaking temperature
Rate decline is obvious.
The food of the most suitable 3% acetic acid additional amount heated at constant temperature under the water-bath soaking temperature of most suitable food will be added, not
With time 1-60 minute sample detection, the aluminium leaching content of sample is observed, selects the heating time of most suitable food, i.e., 30 minutes, is tied
Fruit sees Fig. 6, and soaking time is in 1~30min, the extension at any time of aluminium leaching rate and increase, soaking time is 30~60min
Interior, with the extension of soaking time, the leaching rate of aluminium tends to be steady.
Five, the application of instant test paper of the present invention aluminium element content in detection food (such as jellyfish sample)
It will be added to the water after the chopping of 5g jellyfish, the ratio g:mL of jellyfish and water is 1:9, and adding percentage by volume is 3%
Acetic acid 5mL；With 40 DEG C of water-bath heat 30 minutes after take impregnate drop on test paper, observing response area color, and with standard ratio
Colour atla comparison realizes detection to aluminium content according to the depth of color, the aluminium element content in the food of detection it is whether qualified according to
Judged according to the regulation of national standard, such as aluminium content is more than 100mg/kg, it is as unqualified.
Comparing embodiment: the aluminium content in the method detection jellyfish sample of the prior art is utilized
1) test paper prepare: selections filter paper be test paper material, placement soak (50 DEG C of soaking temperature of 1.5g/L chromazurine s),
It is dried after impregnating 5h.
2) standard color comparison card makes: 0,0.1,0.25,0.5,1,3mL Al standard solution (0.1g/L) is drawn respectively, to
0.2g/L brocide solution 1mL, 10.0g/L ascorbic acid 2mL is added in each pipe and is settled to 10mL.System is taken respectively
Standby series of concentrations aluminum standard solution and the test-paper that 1) step prepares carry out chromogenic reaction.Color is observed after 1min at room temperature
Variation, photographs to record experimental result with digital camera, marks out corresponding Al concentration, standard color comparison card is made in colour print.
3) jellyfish sample detection: by jellyfish with deionized water immersion 10 minutes or more, jellyfish sample liquid is obtained, jellyfish sample is taken
Product liquid successively mixes well to obtain solution to be measured with brocide and ascorbic acid solution, and solution to be measured is added drop-wise to
1) on the test paper of step preparation, it is made to carry out chromogenic reaction with detection paper of aluminum,test piece, by the test paper and standard color comparison card after reaction
It compares, the concentration of Al directly in reading prepare liquid.The recovery of standard addition for obtaining jellyfish sample is 85.1%-127.8%, right
The detection of aluminium obtains the R after two methods detected value linear fit afterwards compared with ICP-MS method in prepare liquid2=0.8243.
Jellyfish sample is detected with test paper of the present invention, show that the recovery of standard addition of sample is 94.6%-105.8%, to leaching
Steep the detection and the ICP-MS method result goodness of fit with higher of aluminium in liquid, the equation after two methods detected value linear fit
Are as follows: Y=1.0159x-0.0724, R2=0.9624.
To sum up, the method for this instant test paper detection Aluminum Content in Food mentions significantly compared with the method for comparing embodiment
The detection range and accuracy rate of aluminium element in high food samples.
Claims (6)
1. a kind of instant test paper of rapid evaluation aluminum in food constituent content, it is characterised in that: making step is as follows:
(1) prepare 1% sulfuric acid solution: drawing 1mol/L sulfuric acid and be diluted with water, until the body that sulfuric acid accounts for overall solution volume is added
Product percentage is 1%, obtains 1% sulfuric acid solution；
(2) prepare acetic acid-sodium acetate solution: weigh the sodium acetate mass concentration soluble in water to sodium acetate be 0.075~
Then glacial acetic acid is added in 0.076g/mL, adjust pH to 5-5.5, and the mass concentration for being then diluted with water to sodium acetate is 0.068g/
ML obtains acetic acid-sodium acetate solution；
The sodium acetate: the ratio g:mL of glacial acetic acid is 17:1.3-1.5；
(3) prepare 3% acetic acid solution: drawing glacial acetic acid and being slowly added into ultrapure water to the percentage by volume of glacial acetic acid is 3%,
Then it mixes, obtains 3% acetic acid solution；
(4) prepare cetrimonium bronmide solution: weighing cetrimonium bronmide and be diluted with water to hexadecyl
The concentration of trimethylamine is 0.2-0.25g/L, obtains cetrimonium bronmide solution；
(5) prepare chrome azurol S solution: weighing chrome azurol S and being diluted with water to the concentration of chrome azurol S is 0.5-0.6g/L, obtains chromazurine
S solution；
(6) the production of colour developing test paper: by 1% sulfuric acid solution, acetic acid-sodium acetate solution, 3% acetic acid solution, cetyl
Base trimethylamine solution, chrome azurol S solution are mixed and made into soak according to the ratio that volume ratio is 1:5:1:1:1, by test paper carrier
It is cut into the long width that multiplies to impregnate in soak 3-5 hours for the rectangle of 4.5-5.5cm × 0.8-1.2cm, 50 DEG C of vacuum constant temperatures are dry
Dry 4h saves, obtains colour developing test paper；
The test paper carrier is chromatography filter paper；
(7) the production of standard color comparison card: by the aluminum standard solution drop of various concentration on colour developing test paper, chromogenic reaction occurs 1-3 points
Zhong Hou takes color with color difference meter, standard color comparison card is made；
(8) up to instant test paper.
2. the instant test paper of rapid evaluation aluminum in food constituent content according to claim 1, it is characterised in that: production
Steps are as follows:
(1) prepare 1% sulfuric acid solution: drawing 1mol/L sulfuric acid and be diluted with water, until the body that sulfuric acid accounts for overall solution volume is added
Product percentage is 1%, obtains 1% sulfuric acid solution；
(2) prepare acetic acid-sodium acetate solution: weigh the sodium acetate mass concentration soluble in water to sodium acetate be 0.075~
Then glacial acetic acid is added in 0.076g/mL, adjust pH to 5.5, and the mass concentration for being then diluted with water to sodium acetate is 0.068g/mL,
Obtain acetic acid-sodium acetate solution；
The sodium acetate: the ratio g:mL of glacial acetic acid is 17:1.3；
(3) prepare 3% acetic acid solution: drawing glacial acetic acid and being slowly added into ultrapure water to the percentage by volume of glacial acetic acid is 3%,
Then it mixes, obtains 3% acetic acid solution；
(4) prepare cetrimonium bronmide solution: weighing cetrimonium bronmide and be diluted with water to hexadecyl
The concentration of trimethylamine is 0.2g/L, obtains cetrimonium bronmide solution；
(5) prepare chrome azurol S solution: weighing chrome azurol S and being diluted with water to the concentration of chrome azurol S is 0.5g/L, and it is molten to obtain chrome azurol S
Liquid；
(6) the production of colour developing test paper: by 1% sulfuric acid solution, acetic acid-sodium acetate solution, 3% acetic acid solution, cetyl
Base trimethylamine solution, chrome azurol S solution are mixed and made into soak according to the ratio that volume ratio is 1:5:1:1:1, by test paper carrier
It is cut into the long width that multiplies to impregnate in soak 4 hours for the rectangle of 5cm × 1cm, the dry 4h of 50 DEG C of vacuum constant temperatures are saved, obtained aobvious
Color test paper；
The test paper carrier is chromatography filter paper；
(7) the production of standard color comparison card: the aluminum standard solution of various concentration 0.25g/L, 0.5g/L, 1g/L, 2g/L, 4g/L are dripped
In on colour developing test paper, after chromogenic reaction occurs 1 minute, color is taken with color difference meter, standard color comparison card is made；
(8) up to instant test paper.
3. the user of the instant test paper such as the described in any item rapid evaluation aluminum in food constituent contents of claim 1 to 2
Method, it is characterised in that: steps are as follows:
It is added to the water after food is shredded, the ratio g:mL of food and water is 1:5-12, adds the second that percentage by volume is 3%
The ratio g:mL of acid, the food and acetic acid is 1:1-3；Drop is impregnated aobvious with taking after 30-60 DEG C of water-bath heating 1-60 minutes
Show on test paper, observing response area color, and compared with standard color comparison card, the detection to aluminium content is realized according to the depth of color.
4. the application method of the instant test paper of rapid evaluation aluminum in food constituent content according to claim 3, special
Sign is: the detection method of the aluminum in food constituent content is as follows:
It is added to the water after food is shredded, the ratio g:mL of food and water is 1:9, the acetic acid that percentage by volume is 3% is added,
The ratio g:mL of the food and acetic acid is 1:1；It is taken after being heated 30-50 minutes with 40 DEG C of immersions of water-bath and impregnates drop in display examination
On paper, observing response area color, and compared with standard color comparison card, the detection to aluminium content, detection are realized according to the depth of color
Food in the whether qualified regulation according to national standard of aluminium element content judged.
5. the instant test paper such as the described in any item rapid evaluation aluminum in food constituent contents of claim 1 to 2 is quickly being surveyed
Determine the application in Aluminum Content in Food.
6. the instant test paper of rapid evaluation aluminum in food constituent content according to claim 5 is in quickly measurement food
Application in aluminium content, it is characterised in that: the food is jellyfish or deep-fried twisted dough sticks.
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| CN106442509A (en) * | 2016-11-08 | 2017-02-22 | 湖南省食品质量监督检验研究院 | Quick detection method for aluminiferous additive in food |
| CN109632776A (en) * | 2018-12-19 | 2019-04-16 | 湖北省食品质量安全监督检验研究院 | Fast selective detects the method and kit that aluminium is added in food |
| CN112730392B (en) * | 2019-12-10 | 2023-01-10 | 浙江省农业科学院 | Test strip for rapidly detecting acid value of salad dressing, preparation method and test method |
| CN111239127B (en) * | 2020-03-11 | 2022-04-15 | 漯河医学高等专科学校 | Simple evaluation method for umami intensity of compound umami seasoning |
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